CN117555076A - Preparation method of gas-phase proton exchange lithium niobate long-period waveguide grating - Google Patents
Preparation method of gas-phase proton exchange lithium niobate long-period waveguide grating Download PDFInfo
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- CN117555076A CN117555076A CN202310982337.6A CN202310982337A CN117555076A CN 117555076 A CN117555076 A CN 117555076A CN 202310982337 A CN202310982337 A CN 202310982337A CN 117555076 A CN117555076 A CN 117555076A
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- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005253 cladding Methods 0.000 claims abstract description 34
- 239000010410 layer Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000012792 core layer Substances 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 235000012239 silicon dioxide Nutrition 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 230000003287 optical effect Effects 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000001465 metallisation Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000009489 vacuum treatment Methods 0.000 claims description 2
- 230000004888 barrier function Effects 0.000 claims 1
- 239000012071 phase Substances 0.000 description 13
- 238000009792 diffusion process Methods 0.000 description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000013307 optical fiber Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 238000000137 annealing Methods 0.000 description 5
- 238000004891 communication Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000001259 photo etching Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000008832 photodamage Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
- G02B6/134—Integrated optical circuits characterised by the manufacturing method by substitution by dopant atoms
- G02B6/1345—Integrated optical circuits characterised by the manufacturing method by substitution by dopant atoms using ion exchange
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/122—Basic optical elements, e.g. light-guiding paths
- G02B6/124—Geodesic lenses or integrated gratings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B2006/12035—Materials
- G02B2006/1204—Lithium niobate (LiNbO3)
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Optical Integrated Circuits (AREA)
Abstract
The invention discloses a preparation method of a long-period waveguide grating based on gas-phase proton exchange, which comprises a lithium niobate substrate (5), a cladding waveguide (3), a core waveguide (4), a buffer layer (2) and an interdigital electrode structure (1) from bottom to top; wherein the buffer layer (2) covers the upper surface of the cladding waveguide (3), and the cladding waveguide (3) and the core waveguide (4) are embedded with the upper surface of the lithium niobate substrate (5); the interdigital electrode structure (1) is positioned on the upper surface of the buffer layer (2); the core layer waveguide (4) is embedded in the middle of the cladding layer waveguide. The invention has the advantages of simple process, stable waveguide performance and the like.
Description
Technical Field
The invention relates to the field of integrated optics, in particular to a preparation method of a gas-phase proton exchange lithium niobate long-period waveguide grating.
Background
In the 21 st century, human beings have entered an information new era mainly characterized by information networks, and the requirements of society and science and technology fields for obtaining information, transmitting information, processing information and storing information are increasing, and the original electric network for transmitting information by electric signals cannot meet the requirements of people, so that an optical fiber communication network using photons as an information carrier gradually becomes a research hot spot in the communication network.
With the development of optical communication technology, research on optical communication devices is receiving attention, and optical communication devices based on optical fibers are greatly developed in terms of device types, manufacturing technologies, application and the like, and particularly in recent years, application and manufacturing technologies of optical fiber gratings are attracting great attention, such as filter design and sensor manufacturing based on optical fiber gratings. However, the optical fiber is relatively fixed in material selection and geometric dimension, so that the flexibility of the design of the optical fiber grating device is limited, and in the aspect of material selection, the waveguide grating can select almost all waveguide materials, such as semiconductors, glass, polymers, lithium niobate and the like, and has good application prospects in the aspects of optical integration and wavelength division multiplexing systems because the waveguide grating has the advantages of small volume, high diffraction efficiency, capability of performing real-time processing, narrow-band filtering, small influence by temperature and the like.
Lithium niobate (LN, liNbO) 3 ) The crystal has been widely studied in terms of manufacturing and application of optical devices due to advantages of good electro-optical effect, easy growth, good thermal stability and the like. The current method for preparing lithium niobate waveguide by titanium diffusion and annealing proton exchange technology is quite mature and is applied to industrial production. The titanium diffusion method is a method for forming a waveguide-shaped titanium strip on the surface of a lithium niobate substrate through the steps of photoetching, coating, stripping and the like, and then forming an optical waveguide through high-temperature diffusion, and the optical waveguide prepared by the process has lower photodamage resistance; the proton exchange is to form a proton exchange area on the surface of lithium niobate after photoetching, coating and stripping, then to carry out proton exchange in weak acid and finally to anneal to form an optical waveguide. The mature preparation process of the lithium niobate waveguide lays a good foundation for the preparation of the waveguide grating.
Since the principle of long period gratings is to couple the core mode with the co-propagating cladding mode at a specific wavelength (resonant wavelength), the core mode energy is coupled into the cladding such that the core energy is attenuated at the specific wavelength. The long period grating requires an optical waveguide with a cladding structure, in which there is no need for additional fabrication because there is a cladding and a core in the structure of the fiber itself to confine the optical energy to be transmitted in the core, but in the long period waveguide grating, there is a need to specially fabricate an optical waveguide with a cladding structure. Since lithium niobate crystals themselves have a large refractive index, it is difficult to find a suitable material as its cladding, and long-period waveguide gratings based on lithium niobate optical waveguides have not been developed until recently. In 2008, a new method for preparing an optical waveguide with a cladding structure on a lithium niobate crystal by using a method of two proton exchange was proposed for the first time by W.Jin, K.S.Chiang et al. The article firstly puts the whole lithium niobate sample into proton exchange liquid to implement surface proton exchange to obtain a slab waveguide, then utilizes a photoetching process to protect the slab waveguide, only carries out proton exchange on partial areas, and obtains the strip waveguide in the areas on the slab waveguide. Wherein, the slab waveguide is used as a cladding layer, and the strip waveguide is used as a core layer to jointly form a special optical waveguide structure. However, the two proton exchange methods increase the complexity of the process, the cladding region is in the annealing diffusion process in the secondary exchange process, the refractive index can be changed again, and in order to improve the refractive index of the core layer, the secondary exchange is often performed by using a pure proton source, the crystal structure of the core layer region is further damaged by the stronger acidity of the secondary exchange, the problems of reduced electro-optic coefficient, increased transmission loss and the like are caused, and the problems limit the further development of the long-period waveguide grating in the fields of optical filters, sensors, optical modulators and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a long-period waveguide grating of gas-phase proton exchange lithium niobate, which adopts a gas-phase proton exchange technology, and a core layer and a cladding layer of a strip waveguide grating can be formed through one-time exchange, so that the problems of complex process, unstable refractive indexes of the core layer and the cladding layer and the like caused by the conventional secondary proton exchange or secondary titanium diffusion process are solved, and the performance of the long-period waveguide grating is further improved. The current manufacturing method of the lithium niobate long-period waveguide grating adopts a proton exchange method or a titanium diffusion method, the temperature of proton exchange is generally over 200 ℃, and the time is generally 1-20H; titanium diffuses at 1100 c for times typically exceeding 40H. Because long period gratings require cladding and core layers with close refractive indices, two waveguide layers are required to be fabricated, and a large-scale cladding layer (typically a slab waveguide) is fabricated for the first time; in order to make the refractive index of the strip waveguide larger than that of the slab waveguide, the slab waveguide subjected to the first exchange is often required to be annealed to reduce the refractive index of the strip waveguide, and steps are added in the two exchanges and annealing, so that the processing difficulty of the device is further increased. To solve this problem, we use a method that allows a cladding and core with close refractive indices to be obtained in one exchange. In the proton exchange experiment, if the temperature is increased to more than 250 ℃, the proton source will become gaseous, the exchange time will generally reach tens to tens of hours, the silicon dioxide mask used in the exchange process will be eroded under the high acid pressure for a long time, and strong lateral diffusion occurs, so that the exchange area is increased, and experiments prove that the phenomenon has an opening time, that is, only exceeds a specific exchange time. By using the phenomenon, a silicon dioxide mask with specific thickness and exchange conditions can be designed, so that the purpose of forming two areas with different refractive indexes through one exchange can be achieved.
The proton source of gas phase proton exchange is gaseous, and a graded refractive index is often formed in the early stage of exchange, as shown in fig. 1; when a certain exchange time is reached, the refractive index of the material will reach a maximum value and the exchange depth will gradually deepen as the exchange time increases, as shown in fig. 2.
When the silicon dioxide layer with the waveguide pattern is contacted with the gaseous proton source, the refractive index is gradually increased, and then the silicon dioxide layer is diffused to the depth direction after reaching the maximum value of the refractive index and keeps the refractive index unchanged, at the moment, the silicon dioxide layer is unchanged, the exchange area is a waveguide core layer area, and the refractive index is recorded as n core . When a certain period of time (13H observed under experimental conditions) is exceeded, large-area lateral diffusion starts to occur, and as shown in FIG. 3, the exchange region expands to the waveguide cladding region, and the refractive index gradually increases due to the initial stage of the exchange, and the exchange is performed for a short period of time, thereby obtaining a refractive index n clodding Is a waveguide cladding region (n) core ＞n clodding ). Experiments show that 13H is the opening time of the phenomenon; thickness of the silicon dioxide layer, pickling time of the earlier silicon dioxide layer corrosion process and annealing condition of the silicon dioxide layerThe lateral diffusion speed is affected, and the current experimental results show that: the silicon dioxide layer with the thickness of 80nm is pickled for 30min, and the maximum transverse diffusion speed can be obtained after annealing for 4h at the temperature of 350 ℃.
From the earlier exchange results, n core In TM 0 The refractive index of the mode is 2.220489, n clodding In TM 0 The refractive index of the mode can be controlled between 2.14581 and 2.21409 by the phase matching condition λ=Λ (n core -n clodding ) When λ=1550 nm, the grating period that can be satisfied is 20 to 240 μm.
Drawings
FIG. 1 is a graph of the graded index profile of a gas phase proton exchange system according to the present invention;
FIG. 2 is a graph of the gas phase proton exchange step index profile of the present invention;
FIG. 3 is a waveguide microscope image of the lateral diffusion phenomenon referred to in the present invention;
FIG. 4 is a schematic diagram of a vapor phase proton exchanged lithium niobate long period waveguide grating according to the present invention;
FIG. 5 is a schematic diagram of a core waveguide of a method for fabricating a gas-phase proton exchanged lithium niobate long-period waveguide grating according to the present invention;
FIG. 6 is a schematic diagram of a cladding waveguide of a method for fabricating a gas-phase proton exchanged lithium niobate long-period waveguide grating according to the present invention;
reference numerals: 1. the electrode comprises an interdigital electrode, 2 parts of buffer layers, 3 parts of cladding waveguides, 4 parts of core waveguides, 5 parts of lithium niobate substrates, 6 parts of silicon dioxide masks.
Detailed Description
The technical scheme of the invention is described in detail below with reference to the accompanying drawings and specific embodiments.
As shown in fig. 4, a schematic diagram of a gas-phase proton exchange lithium niobate long-period waveguide grating according to the present invention includes an interdigital electrode 1, a buffer layer 2, a cladding waveguide 4, a core waveguide 3, and a lithium niobate substrate 5. The upper surface of the cladding waveguide 4 is covered with a buffer layer 2 and embedded in a lithium niobate substrate 5; the upper surface of the buffer layer 2 is covered with the interdigital electrode 1; the core layer waveguide 3 is embedded in the middle of the upper surface of the cladding flat waveguide 4; and voltage is applied to the core layer waveguide through the interdigital electrode structure, so that the distribution of the refractive index of the crystal in the waveguide direction is changed, and the core layer 3 is optically coupled into the cladding slab waveguide 4.
All electrodes can be made of metal materials with good conductivity such as gold; the width W of the interdigital electrode 1 is 5-20 mu m, the length L is 10-30 mm, and the thickness H is 5-30 mu m; the interval between the interdigital electrodes is 10-30 mm.
The buffer layer 2 is made of silicon dioxide material.
The core layer waveguide 3 adopts proton exchange strip waveguide with width T of 5-10 μm and refractive index n core The method comprises the steps of carrying out a first treatment on the surface of the The cladding waveguide 4 adopts proton exchange strip waveguide with the width T of 500-2000 μm and the refractive index n cl odding，n core ＞n clodding 。
The invention relates to a preparation method of a gas-phase proton exchange lithium niobate long-period waveguide grating, which comprises the following steps:
step 1, sample preparation, which specifically comprises the following steps: selecting a lithium niobate wafer as an initial material, and cutting the wafer into waveguide samples by using a precision cutting machine;
step 2, manufacturing a waveguide mask, which specifically comprises the following steps: plating a layer of silicon dioxide mask on the surface of the sample; manufacturing a waveguide pattern on the silicon dioxide layer by using photoetching and etching processes, so that the silicon dioxide is not covered on the waveguide, and the rest parts are still covered with the silicon dioxide, so that a waveguide sample is clear and clean;
step 3, proton exchange is carried out, and the step specifically comprises the following steps: placing the exchange buffer medicine and the waveguide sample in a reaction crucible, performing high vacuum treatment by using a vacuum pump, forming a high vacuum negative pressure state in the crucible, placing the reaction crucible in an exchange furnace, heating to exchange temperature and keeping constant temperature for 8-18H, and forming a core layer waveguide by no change of mask patterns when the exchange time is less than 13H, as shown in figure 5; when the exchange time exceeds 13H, the lateral diffusion starts to appear under the influence of high-pressure benzoic acid gas in the crucible, so that the exchange area is enlarged, and a cladding waveguide is formed, as shown in FIG. 6; the exchange temperature exceeds 300 ℃;
step 4, polishing the end face;
step 5, performing alignment of interdigital electrode patterns according to the alignment mark of the waveguide layer, performing metallization treatment on the aligned sample, and manufacturing a metal interdigital electrode with the thickness of 500 nm-8 mu m by using a stripping process;
through the steps, the long-period waveguide grating based on gas-phase proton exchange is prepared, so that the core-layer waveguide and the cladding-layer waveguide with different refractive indexes can be obtained through single preparation, the process is simple, and the refractive index is stable.
The electrode structure in the invention can also adopt traveling wave electrodes and the like, and the technical scheme of the invention is utilized, or a similar technical scheme is designed by a person skilled in the art under the inspire of the technical scheme of the invention, so that the technical effects are achieved, and the technical effects fall into the protection scope of the invention.
Claims (4)
1. The long-period waveguide grating is characterized in that the waveguide grating structure comprises a lithium niobate substrate (5), a cladding waveguide (3), a core waveguide (4), a buffer layer (2) and an interdigital electrode structure (1) from bottom to top; wherein the buffer layer (2) covers the upper surface of the cladding waveguide (3), and the cladding waveguide (3) and the core waveguide (4) are embedded with the upper surface of the lithium niobate substrate (5); the interdigital electrode structure (1) is positioned on the upper surface of the buffer layer (2); the core layer waveguide (4) is embedded in the middle of the cladding layer waveguide.
2. A long period grating according to claim 1, characterized in that the core waveguide (4) is a gas phase proton exchange strip waveguide.
3. A long period grating according to claim 1, characterized in that the cladding waveguide (3) is a gas phase proton exchange strip waveguide.
4. A method of waveguide preparation of a gas phase proton exchanged long period waveguide grating according to claim 1, comprising the steps of:
step (1) of sample preparation, which specifically comprises the following steps: selecting an optical grade lithium niobate wafer as an initial material;
step (2), manufacturing a waveguide mask, wherein the material of the waveguide mask is silicon dioxide, and the waveguide mask is used as an exchange barrier layer;
step (3) of proton exchange, which specifically comprises the following steps: placing the exchange buffer medicine and the waveguide sample in a reaction crucible, performing high vacuum treatment by using a vacuum pump, forming a high vacuum negative pressure state in the crucible, placing the reaction crucible in an exchange furnace, heating to exchange temperature and keeping constant temperature for 8-18H, and tightly attaching the edge of the waveguide pattern on the silicon dioxide layer to the lithium niobate wafer without changing the mask pattern when the exchange time is less than 13H; when the exchange time exceeds 13H, the edge of the waveguide pattern on the silicon dioxide layer starts to be separated from the lithium niobate wafer under the influence of high-pressure benzoic acid gas in the crucible, so that the exchange area is enlarged, and secondary exchange is formed; the exchange temperature exceeds 300 ℃;
step (4), polishing the end face;
step (5), performing alignment of the interdigital electrode patterns, and manufacturing metal interdigital electrodes by using a stripping process after metallization treatment;
through the steps, the core layer waveguide (4) and the cladding layer waveguide (3) based on gas-phase proton exchange and the interdigital electrode structure (1) are prepared.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310982337.6A CN117555076A (en) | 2023-08-07 | 2023-08-07 | Preparation method of gas-phase proton exchange lithium niobate long-period waveguide grating |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310982337.6A CN117555076A (en) | 2023-08-07 | 2023-08-07 | Preparation method of gas-phase proton exchange lithium niobate long-period waveguide grating |
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| CN117555076A true CN117555076A (en) | 2024-02-13 |
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| CN202310982337.6A Pending CN117555076A (en) | 2023-08-07 | 2023-08-07 | Preparation method of gas-phase proton exchange lithium niobate long-period waveguide grating |
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- 2023-08-07 CN CN202310982337.6A patent/CN117555076A/en active Pending
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